Azobisisobutyronitrile → HCID 86725430, 화합물

HRID 1525920노트

반응식

HRID 1525920 반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9]([O:11][CH2:12][CH3:13])=[O:10])=[C:4]([F:14])[CH:3]=1.[Br:15]N1C(=O)CCC1=O.N(C(C)(C)C#N)=NC(C)(C)C#N>C(Cl)(Cl)(Cl)Cl>[Br:15][CH:8]([C:5]1[CH:6]=[CH:7][C:2]([Br:1])=[CH:3][C:4]=1[F:14])[C:9]([O:11][CH2:12][CH3:13])=[O:10]

참가 물질

5

반응물 3

HCID 6547AzobisisobutyronitrileHCID 67184N-bromobutanimideHCID 45790370Ethyl (4-bromo-2-fluorophenyl)acetate

생성물 1

HCID 86725430HCID 86725430, 화합물수율 96.1%

시약·촉매·용매 1

HCID 5943Carbon Tetrachloride용매

반응 조건

온도
90 °C

실험 절차

To a stirring solution of ethyl 2-(4-bromo-2-fluorophenyl)acetate (3.92 g, 15.0 mmol) in carbon tetrachloride (50 mL) was slowly added N-bromosuccinimide (2.67 g, 15.0 mmol) and then azobisisobutyronitrile (0.37 g, 2.3 mmol). The reaction mixture was stirred for 9 h at 90° C. and then cooled to room temperature. The residue was purified by flash chromatography (0-100% ethyl acetate/hexanes) to provide the title product (4.9 g, 96% yield). MS(ES)+ m/e 340.9 [M+H]+.

후처리

  1. temperaturecooled to room temperature
  2. customThe residue was purified by flash chromatography (0-100% ethyl acetate/hexanes)

출처 및 근거

ORD 기록
ord-6db28024aaea44daa019a47408d72cb8
출처 데이터셋
uspto-grants-2015_07
특허 번호
US09084794B2

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